ES2246316T3 - GEL COMPOSITIONS. - Google Patents

Abstract

The invention relates to a composition which comprises a dispersion of micro spheres in a gel comprising an oily base and an organic polymeric gelling agent.

Description

Gel compositions.

This invention relates to gel compositions. containing microspheres for filling cables, such as cables of communication, and methods to prepare such gels.

Background of the invention

Communication cables typically comprise a core that conducts the signal surrounded by a protective sheath. The core, for example, can conduct light signals or electrical signals. In many cables, the space between the conductor and the sheath contains a padding, whose function is to protect and cushion the core from external forces that could occur, for example, when bending or winding, particularly in the case of fiber cables optics. A further function of the landfill is the prevention of water ingress that is particularly relevant when the core comprises a metal such as copper. To meet these requirements, the padding must show several features. The filling must be of sufficient viscosity to allow lateral movement of the core that occurs, for example, when bending, rolling or tracing. The viscosity, however, should not be so low to allow a drip loss of the filling during vertical cable routing. In addition, this balance of properties must be maintained in a temperature range of -40 to + 80 ° C. The filler must be formulated to be chemically compatible with cable quality polymers, which include not only the cable sheath, but also coatings typically found in optical fibers. The padding must also show a high degree of elasticity to absorb the force of impacts that the cable sheath may suffer during its operational life. Relatively high ambient temperatures can be achieved by the manufacture of such cables causing thermal expansion of the landfill which then leads to the formation of holes and cavities upon cooling. Such holes and cavities can potentially become a path for water that in fiber optic cables can lead to the attenuation of the light wave guide. Therefore, cable fillers should ideally show low thermal conductivity. For electrical applications or for cores that transmit electrical signals, it is advantageous that the filling has a low permittivity so that the conduction core is isolated. This has the additional advantage of providing a hydrophobic filler that thus protects the core from the water inlet. The drip resistance of the fillers can be improved by reducing their specific weight. Finally, for easy handling, it is preferred that the filling is semi-dry to the touch, rather than
sticky.

Existing fillers used in cables Telecommunications include oil gels that are primarily mixtures of oils and gelling agents. In your application, penetrate between the beams of, for example, copper conductors densely packed insulated and thus isolate them from moisture. He oil, which comprises a main part of the mixture, can be a naphthenic or paraffinic processing oil, an oil mineral, a synthetic product such as a polybutane or an oil of silicone. The gelling agents include waxes, silicic acids (silica gels), pyrogenic silica, fatty acid soaps and thermoplastic elastomers. Typically the gelling agent It comprises less than 10% of the total.

A particular family of elastomers thermoplastics marketed under the trademark "Kraton" (Shell Chemical Company), includes configurations molecular di-block, tri-block or multi-branched polystyrene segments and rubber.

US 5,657,410 describes an element of optical transmission that includes a filler comprising between 80% and 95% by weight of a monomeric plasticizer having a weight molecular in the range of 200-2000 grams per mol. Such monomeric plasticizers include phthalate esters, trimellitatos, phosphates and fatty esters. Can also be added additional substances such as thickeners. He Thickener can take the form of small spheres. Spheres Hollow are preferred due to its great compressibility and easy processibility Agents can also be added advantageously. thixotropic They include finely divided or pyrogenic silica, alumina, and bentonites as well as mixtures of these substances.

The use of microspheres, for example hollow microspheres, in cable filling compounds is also described in US 5,698,615. In this description the cable filling comprises a substantially dry hydrophilic composition containing, among other things, in addition to the microspheres, water-absorbable inflatable powder particles, preferably of a particle size in the range of 1-30 µm and a " sprinkle powder "which has particles preferably a fraction 1/100 of the size of the inflatable powder particles. Due to the hydrophilic nature of the inflatable powder particles, the composition always retains some water. Dusting powder particles are arranged between the inflatable powder particles to prevent agglomeration when the swellable polymer particles absorb water. Suitable inflatable powder particles are those based on the sodium salt of polyacrylic acid. The powdered particles sprinkled are typically inorganic powders such as talc, mica, graphite and silicates. The absorption of water by the inflatable powder particles transforms the dry composition into a gel that seals the core of the entrance of more water. The compositions may also contain a small amount of an oil or an adhesive to reduce any risk of dust.
potential.

WO 99/15582 describes a composition which includes expandable hollow microspheres for use in encapsulation of, for example, semiconductor chips. Such hollow microspheres, similar in morphology to microspheres described in US 5,657,410 and US 5,698,615, comprise a polymeric housing that encapsulates a blowing agent. When heats up, the polymeric shell of the expandable microspheres is gradually softens and liquid blowing agent, typically isobutane, begins to evaporate expanding the microsphere.

A light wave guide conductor is described in US 5,335,302 comprising at least one waveguide luminous accommodated in a protective sheath and embedded in a pasty filler material that contains small microspheres. The small microspheres, which can be solid and rigid, solid and elastic or hollow and elastic, are included as fillers for reduce cost, and provide better rheological properties and shock absorbers A preferred filler comprises an oil, an agent thixotropic (for example, fumed silica) and an organic thickener not specified.

Summary of the invention

In one aspect, the present invention provides a composition, particularly a composition suitable for use as a cable filling, comprising a dispersion of microspheres expanded hollows in a gel comprising an oily base and a thermoplastic elastomer. In which the microspheres have each one, a housing formed of an acrylonitrile copolymer and meta-acrylonitrile with a number in the "Chemical Abstract "from 38742-70-0.

Preferably the composition is substantially free of silica, for example pyrogenic silica.

The gels of the invention may also contain an antioxidant

The oily base may comprise an oil of hydrocarbon or a silicone oil. Hydrocarbon oils particularly preferred include white mineral oils and synthetic poly (α-olefin) oils. The oily base typically constitutes 1-99% in gel weight, more preferably 50-99% by weight of the gel, in particular 80-99% by weight of the gel.

Examples of thermoplastic elastomers include thermoplastic rubbers. The thermoplastic elastomer can be a copolymer, for example a block copolymer that has a molecular configuration of di-block, tri-block, or multi-branched. In a particular embodiment, the blocks are comprised of rubber or polystyrene. The rubber can be an olefin rubber saturated composed of monomer units of ethylene, propylene or butylene Alternatively, the rubber may be a rubber of unsaturated olefin comprising butadiene monomer units or isoprene.

Particular examples of elastomers thermoplastics include tri-block copolymers from styrene-ethylene / butylene-styrene (SEBS), di-block copolymer of styrene-ethylene / propylene (SEP), copolymer multi-branched ethylene / propylene (EP), tri-block copolymer of styrene-butadiene-styrene (SBS) and tri-block copolymer of styrene-isoprene-styrene (SIS).

The thermoplastic elastomers available in the Trade includes the copolymers available under the brand Shell's "Kraton" commercial.

The thermoplastic elastomer is typically used in the proportions in the range of 1-10% by weight of the composition, more preferably in the range of 2-9% by weight of the composition, in particular in the range of 3-8% by weight of the composition.

The invention uses compressible hollow microspheres each comprising a polymeric housing that encapsulates a blowing agent. The polymeric shell is formed of a copolymer, according to claim 1. The blowing agent, for example, can be isobutane or isopentane. In addition, the microspheres are expanding
you give.

Such hollow microspheres show a high degree of elasticity and also have a low specific weight. The use of such microspheres in the gels described in this invention is advantageous because they reduce the total specific weight of the gels and therefore reduce or eliminate dripping during vertical tracing of the cable.

The hollow nature of the microspheres means that the proportion of solid material is very low in relation to the volume. Thus, its addition to the gels of the invention leads to a reduction of total thermal conductivity and to a probability less decomposition of any of the gel components or to the creation of gaps at the high temperatures reached during cable manufacturing. Elastic properties superiors of hollow microspheres over their solid competitors provide better protection to, for example, waveguides bright during transport, rolling or tracing. Further, the problem of attenuation of the guides of light waves due to the presence of holes or cavities inside of the cable filling when any increase in the volume of the thickness of the filling is reached due to heating during cable manufacturing for an opposite reduction in the volume of hollow microspheres Due to the compressible nature of such hollow microspheres, their typical diameters are larger than those of Your solid competitors. In fiber cable applications optics, diameters in the diameter range of The light wave guide. The diameters of the hollow microspheres expanded will typically be in the range of 1-200 µm, more generally in less than 100 um, typically in less than 75, for example 15 to 55 \ mum.

The hollow microspheres that are used are typically present in the range of 1-95% v / v, more preferably 5-95% v / v, in particular 50-95% v / v, referring to the preceding figures to Expanded volumes

The antioxidant can be selected from the commonly used in the art. Phenolic antioxidants are the preferred ones The antioxidant is typically present in a amount of 0.01-1% w / w, for example of 0.1-1% w / w

In a further aspect, the invention provides a Composition as defined earlier in this document for use as cable filling.

In another aspect, the invention provides a cable, such as a communications cable, that contains a filler as defined earlier in this document.

In yet another aspect, the invention provides a cable comprising a conduction core surrounded by a sheath, a composition as defined above in this document being arranged between the conduction core and the sheath. The conduction core can be, for example, a driver electric or a light conductor. The electric conductor can be, for example, a conductor to conduct electrical signals such Like telephone signals.

In a further aspect, the invention provides a method for preparing a cable comprising a core of conduction and a sheath, the process comprising the stage of Extrude the cable sheath into the conduction core and interpose a composition as defined earlier in this document between the conduction core and the sheath during the stage of extrusion.

In another aspect, the invention provides a procedure for preparing a gel as defined above in this document; Understanding the procedure:

(to)

heat the oily base to a temperature in the range of 110 ° C to 120 ° C;

(b)

add thermoplastic elastomer to the oily base and mix to form a mixture;

(C)

cool the mixture to a temperature of less than 90 ° C;

(d)

add and mix in the microspheres; and optionally

(and)

add and mix in an antioxidant; I

(F)

keep the mixture under vacuum to Remove trapped gas.

In a preferred embodiment, the process understands:

(i)

mix at least one oil in a heating-mixing tank;

(ii)

heat the mixed oils to 110-120 ° C in a stirred tank of heating-mixing;

(iii)

add and mix the elastomer thermoplastic to the oily base with high shear for no more than one hour after transferring the oily base to a tank of mixing-cooling, allowing the temperature of the mixture rises to more than 120-130 ° C;

(iv)

cool the mixture to <90 ° C and transfer it to a stirred main reactor,

(v)

add and mix a antioxidant;

(saw)

add and mix the microspheres, extracted to the reactor under vacuum or pumping, for at least two minutes;

(vii)

keep the vacuum for at least another 10 minutes to remove bubbles air before releasing the finished gel.

Although the temperature of the mixture is typically <90 ° C after cooling, more preferably it is <80ºC, in particular it is <70ºC.

Other aspects and particularities of the invention are as set forth in the claims added in this document.

Brief description of the drawings

The invention will now be illustrated, but not limited, as for the particular embodiments shown in the accompanying drawings, in which:

Figure 1 shows a cross-sectional view of a electric cable; Y

Figure 2 shows a cross-sectional view of a optical cable;

Figure 3 is a plot of viscosity versus at the shear rate for the composition of Example 1 at 25 ° C; Y

Figure 4 is a graph of viscosity versus the shear rate for the composition of Example 2 a 25 ° C

Detailed description of the preferred embodiments

Figure 1 shows a cross-sectional view of a electric cable 11, comprising, in this example, four electrical conductors 13 coated in the liner 12. The electrical conductors 13 themselves comprise a conductor electrical 14, preferably copper, and an external insulation 15,  typically polyethylene. Scattered among the drivers electrical 13 and the outer lining 12, there is a composition 16 of filling gel. In this embodiment, the filling composition it can comprise an oily base, a thermoplastic rubber such as a thermoplastic elastomer and dispersed microspheres and optionally an antioxidant. The electric cable, comprising typically a copper core, can be used for the purposes of telecommunications or electricity distribution.

Although Figure 1 shows a cross-sectional view of an electric cable comprising four conductors in a star quad configuration, it will be appreciated that wires that have a variety of different configurations can be used as alternatives to the configuration shown.

Figure 2 shows an optical cable 21 that comprises three coated 23 fiber optic buffer tubes in the coating 22. The fiber optic buffer tubes 23 they consist of an optical fiber 24 provided with a protective coating 26 and a protective sheath 25. The composition of filler 27 is disposed between the covered optical fiber and the protective sheath In addition, fill in the interstices formed between the individual buffer tubes and between the tubes shock absorbers and the inner surface of the lining of the cable.

Examples of specific gels suitable for use in cables, such as the cables illustrated in Figures 1 and 2, are as follows:

Example 1

A gel filling was prepared having the following composition:

Component Concentration (% by weight) Mineral oil White 89.0 SN 500 (Mobil) Elastomer thermoplastic 5.5 Kraton 1701 or 1702 (Shell) Microspheres (pre-expanded) 5.0 Expancel 091 DE (Triones Chems. Int.) Antioxidant 0.5 Irganox L 135 (Ciba-Geigy)

The gel filling of this example is suitable to fill the interstices between the pipes and conductors (of high lighting) and is not in direct contact with the guides fiber.

The gel was prepared as follows:

The oily base was introduced in a tank stirred heating-mixing and was heated to 110-120 ° C before transferring it to a tank of high shear mixing-cooling, to which it was added thermoplastic elastomer (Kraton) (in the form of granules). The mixture was mixed under high shear conditions using multitasking immersion mixing emulsifier (Silverson Machines Limited, Model GDD 25) for no more than 60 minutes During the mixing procedure, the Mix temperature rises to 120-130 ° C. The mixture was cooled by a cold water cooling system, and the cooled mixture was transferred to a stirred main reactor where the antioxidant was added. Then the void was created inside the reactor to aspirate the microspheres that were mixed in the mixture for a period of at least two minutes. He vacuum was maintained for at least ten more minutes to effect the elimination of any air bubble. The emptiness then was released, the stirrer was turned off and samples were taken before of releasing the finished gel from the main reactor.

The product was characterized by several analysis, the results of which are summarized in Table 1 then. The thermal conductivities referred to in the table were determined as follows:

The disks of the test sample were created by collecting the gels in a pair of nylon rings in diameter medium internal 70.1 mm and average thickness 10.03 mm and placing adhesion film above and below. A small correction was made to have a supplementary interface introduced by the adhesion film The thermal conductivity of the samples of test was measured using a 76-degree safety heating plate mm A pair of disks from the test sample were mounted, under the pressure of two cooled plates, on each side of the plate safety heater. The cooled plates were maintained at a constant temperature of ± 0.05 ° C. The surfaces of the plates had 0.9 emitters. The annular safety temperature on the heating plate was adjusted with that of the central part to ± 0.01 ° C to minimize lateral heat flow at The test samples. The heating plate and the samples of test were isolated with a fiberglass blanket to further reduce heat losses from the edge. The fall of the temperatures by the test samples was set at 14 ° C and at approximately 5 hours was allowed to be established on thermal equilibrium before the readings were taken late.

The aging trial was derived from YD / T839.4-1996 (PRC Method) except that they were changed the temperature and the duration of the test.

TABLE 1

Physical Properties Property Value Testing method Density (20ºC) g / ml 0.356 ASTM D 1475 Viscosity (100 s 1, 25 ° C) Pa.s 23.63 Haake VT500 Tube drain (7 mm ID / 80ºC / 24 hours) He passed EIA / TIA-455-81A Cone Penetration (23ºC) dmm 335 ASTM D937 Cone Penetration (-30ºC) dmm 167 ASTM D937 Cone Penetration (-40ºC) dmm 120 ASTM D937 Oil separation (80ºC / 24 hours)% in weight 0 FTM791 (321) Loss of volatiles (80ºC / 24 hours)% in p / p 0.17 FTM791 (321) ILO (190ºC) minutes 34.75 ASTM D3895 Thermal conductivity (23ºC) W / m K 0.077 see above Thermal conductivity (80ºC) W / m. K 0.078 see above Hydrogen generation (80ºC / 24 hours) \ mul / g 0.010 Value MgKOH / g acid 0.036 BS2000 Aging (100ºC / 240 hours) He passed see previous UV exposure (25ºC / 14 days) He passed Exposition of temperatures (240ºC / 5 minutes) He passed ILO = time of oxidative induction

Table 1 shows that the gel density is low what contributed to get good anti-drip properties (measured at 80 ° C). The behavior at low temperatures was evaluated by cone penetration at -40 ° C while the high temperature behavior was analyzed by a combination of the draining technique, the separation test of the oil and volatile loss all carried out at 80 ° C and the oxidative induction time test carried out at 190 ° C. A oxidative induction time greater than 20 minutes is desirable. The results indicate that the gel has a temperature range operating from -40 to + 80ºC. In addition, the rheological behavior of gel, shown in figure 3, is thixotropic (fluidization by shear) allowing cold pumping and processing, and thus the cable filling with the absence of holes created by the gel shrinkage.

The thermal conductivity was determined at 23 ° C and 80 ° C The values for conductivity were low reflecting the low gel density, and varied little with temperature what suggests a material that has a messy structure. The good insulation properties indicated that it was a material that it has good resistance to thermal decomposition that it can occur at high temperatures reached during the cable manufacturing. In addition, the gel would be less sensitive to thermal expansion and contraction that can occur during the cable manufacturing leading to the formation of gaps in the cable filling. For comparison purposes, the thermal conductivities of a range of materials in the Table 2.

TABLE 2

Conductivities Thermal of Various Materials Material Thermal conductivity W / m.K Commentary Aluminum 200 Very good driver Water 0.6 Olive oil 0.17 Paraffin 0.15 Air 0.024 Very good insulator

The gel showed good properties of aging and resistance to UV and temperature. There was also a low generation of hydrogen gas.

Example 2

A similar gel filler was prepared from a similar to that described in Example 1, but with a quality different from mineral oil. The gel was suitable for use in filling and fluidization applications of small cables copper phone pairs.

The gel was subjected to several physical analyzes. The results of the physical analyzes were similar to those of the composition of Example 1 and therefore only the electrical properties in Table 3.

TABLE 3

Properties Physics Property Value Method of test Dielectric constant (23 ° C) 1.62 ASTM D924 Dielectric Dissipation Factor (1 MHz) 4.4 x 10-4 ASTM D924 Volume resistance (23ºC) Ohm.cm 2.8 x 10 15 ASTM D257 Tension kV break 86

The gel is characterized by a low permittivity relative (1.62) and a large volume resistor (2.8 x 10 15 Ohm.cm). For comparison purposes, the relative permittivities of various materials in Table 4.

TABLE 4

Relative Permitivities of Several materials Material Relative permissiveness Air (normal pressure) 1,0005 Paraffin wax 2 Kerosene 4.7 Glass 5-10 Mica 6 Alcohol of methyl 32 Water 81

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Example 3

A gel suitable for use in tube filling baggy and interstitial filling between ribbons and grooved cores open was prepared in a manner similar to that described in the Example 1. The formula for this gel is described below:

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Component Concentration (% by weight) Oil of poly (α-olefin) a 66.37 Durasyn 166 (Amoco) Mineral oil White 22.13 Whiterex 250 (BP / Mobil) Elastomer thermoplastic 7.5 Kraton 1701 or 1702 (Shell) Microspheres (pre-expanded) 3.5 Expancel 091 DE (Triones Chems. Int.) Antioxidant 0.5 Irganox L 135 (Ciba-Geigy) a The oil of poly (α-olefin) also supplies it  BP / Mobil as SHF 61

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The gel was subjected to several physical analyzes. The results of the physical analyzes, which were similar to those Results of the composition of Example 1 are shown in the Table 5.

In addition the resistance limit was analyzed to tensile and breaking stress of fiber lining optics in accordance with FOTP-28 standards and FOTP-178 respectively. The fiber optic was CPC6 manufactured by Siecor. The trials were carried out after of fiber aging in forced air chambers for 30 days at 85 ± 1 ° C immersed in gel. The measures were carried out at 20 ° C and relative humidity of 70%. The limit of tensile strength was measured in thirty 0.5 mm samples from four different groups at an elongation rate of 500 ± 50 mm / minutes. 50 mm samples were used for proof of the coating breaking stress using a 500 ± 50 mm / minute release tool. The values of limit of average tensile strength and stress of coating rupture for a control sample were 68.89 N and 3.61 N respectively.

TABLE 5

Physical Properties Property Value Testing method Density (20ºC) g / ml 0.438 ASTM D 1475 Viscosity (200 s 1, 25 ° C) Pa.s 7.95 Haake VT500 Tube drain (7 mm ID / 80ºC / 24 hours) He passed EIA / TIA-455-81A Cone Penetration (23ºC) dmm 396 ASTM D937 Cone Penetration (-40ºC) dmm 250 ASTM D937 Oil separation (80ºC / 24 hours)% by weight 0 FTM791 (321) Loss of volatiles (80ºC / 24 hours)% in p / p 0.06 FTM791 (321) ILO (190ºC) minutes 31.04 ASTM D3895 Thermal conductivity (23ºC) W / m.K 0.077 see example 1 Thermal conductivity (80ºC) W / m.K 0.078 see example 1 Hydrogen generation (80ºC / 24 hours) \ mul / g 0.015 Relative permittivity (50 Hz, 25 ° C) 1.65 ASTM D150 Volume resistance (23ºC) Ohm.cm 19 x 10 14 ASTM D257 Limit of tensile strength (20ºC / 70% RH) N 65.07 FOTP - 28 Breaking effort of coating (20ºC / 70% RH) N 3.88 FOTP - 178 Aging (100ºC / 240 hours) He passed see example 1 UV exposure (25ºC / 14 days) He passed Exposure to temperatures (240ºC / 5 minutes) He passed ILO = oxidative induction time

The shear sensitive behavior of the viscosity is illustrated in figure 4 and shows that the gel is thixotropic or fluidifiable by shear. This gel although of lower viscosity than the gel of example 1, even passed the test  of drainage. The behavior at low temperatures, characterized by a cone penetration at -40 ° C, it was exceptional. This is particularly important when using this gel in contact direct with optical fibers and should maintain flexibility to low temperatures to avoid applying stress to the fibers previously mentioned or microdoblamientos caused by contractions that can lead to increased attenuation. He tensile strength limit and breaking stress of coating suggested that there was no deterioration in the mechanical resistance of the fibers or degradation in the fiber coating after exposure to the gel.

Claims (14)

1. A composition comprising a dispersion of hollow expanded microspheres in a gel comprising a base oily and a thermoplastic elastomer, in which the microspheres each have a housing formed of a copolymer of acrylonitrile and methacrylonitrile, having a number in the "Chemical Abstract" by 3B742-70-0. 2. A composition according to the claim 1, the composition being substantially free of silica, for example pyrogenic silica. 3. A composition according to the claim 1 or claim 2, wherein the oily base comprises at least one oil selected from naphthenic or paraffinic processing, mineral oil, oils synthetics such as synthetic oil from poly (α-olefin) and oil silicone. 4. A composition according to any one of the preceding claims, wherein the oily base is present in an amount in the range of 1 to 99% by weight of the composition. 5. A composition according to the claim 4, wherein the oily base is present in a amount in the range of 50 to 99% by weight of the composition, per example in the range of 80-99% by weight of the composition. 6. A composition according to any one of the preceding claims, wherein the elastomer Thermoplastic is a thermoplastic rubber. 7. A composition according to any one of the preceding claims, wherein the elastomer thermoplastic is present in an amount in the range of 1-10% by weight of the composition, for example in the range of 2-9% by weight of the composition, preferably in an amount in the range of 3-8% by weight of the composition. 8. A composition according to any one of the preceding claims containing one or more antioxidants 9. A cable, such as a communications cable, containing as filling a defined composition in any of claims 1 to 8. 10. A cable according to claim 9 comprising a conduction core surrounded by a sheath, a composition as defined in any one of the claims 1 to 8 being disposed between the core of driving and sheath. 11. A cable according to claim 9 or claim 10, wherein the conduction core is a electric conductor or a light conductor. 12. A procedure to prepare a cable that it comprises a conduction core and a sheath, comprising the procedure the stages of extruding the cable sheath into the core driving and interposing a composition as defined in a any of claims 1 to 10 between the core of conduction and sheath during extrusion stage. 13. A procedure to prepare a composition as defined in any one of the claims 1 to 8, the process comprising:

(to)

heat the oily base to a temperature in the range of 110 ° C to 120 ° C;

(b)

add thermoplastic elastomer to the oily base and mix to form a mixture;

(C)

cool the mixture to a temperature of less than 90 ° C;

(d)

add and mix the microspheres; Y optionally

(and)

add and mix an antioxidant; I

(F)

keep the mixture under vacuum to Remove trapped gas.

14. A procedure in accordance with the claim 13 for manufacturing a composition according to a any one of claims 1 to 8, the process:

(i)

mix at least one oil in a heating-mixing tank,

(ii)

heat the mixed oils to 110-120 ° C in a stirred tank of heating-mixing;

(iii)

add and mix the elastomer thermoplastic to the oily base with high shear for no more than one hour after transferring the oily base to a tank of mixing-cooling, allowing the temperature of the mixture rise to more than 120-130 ° C;

(iv)

cool the mixture to <90 ° C and transfer it to a stirred main reactor;

(v)

add and mix in a package antioxidant;

(saw)

add and mix the microspheres, extracted to the reactor under vacuum or pump, for at least two minutes;

(vii)

keep the vacuum for at least another 10 minutes to remove bubbles air before releasing the finished composition.